Diamond Annual Review 2019/20
82 83 D I A M O N D L I G H T S O U R C E A N N U A L R E V I E W 2 0 1 9 / 2 0 D I A M O N D L I G H T S O U R C E A N N U A L R E V I E W 2 0 1 9 / 2 0 Soft CondensedMatter Group Robert Rambo, Science Group Leader T he Soft CondensedMatter (SCM) Group provides the Infrared (IR) and Circular Dichroism(CD)microspectroscopy and both Small andWide Angle X-ray Scattering (SAXS and WAXS) capabilities of Diamond Light Source. These capabilities are provided by the four beamlines: High Throughput SAXS (B21), the Multimode Infrared Imaging And Microspectroscopy (MIRIAM) beamline (B22), SAXS and Diffraction (I22) and the CD beamline (B23). This unique portfolio of beamlines can analyse a range of samples that include two-dimensional thin-films (photovoltaics), living mammalian cells, three-dimensional matrices (e.g. metal-organic frameworks, gels and waxes) and nano-particles in non-crystalline states. SCM now offer mail-in services for SAXS and CD measurements through UAS announcements. In addition, I22, B22 and B23 offer off-line access to IRmicroscopy and imaging, CD spectroscopy, and SAXSmeasurements. In the last year, the SCM Group contributed to 132 scientific publications with B21 increasing their publications to a new record of 57. SCM publications include topics such as photo-chemistry examining the stacking arrangements within photosynthetic membranes, light induced chirality in thin-films, the structure of a Type III CRISPR, engineering of metal-organic frameworks for catalysis, the discovery of a new liquid crystalline hexagonal phase and food sciences that showed SAXS has the required sensitivity to follow the early stages of fat crystallization. The SCM group joined with the newly formed UKRI-BBSRC funded FoodBioSystems doctoral training program (DTP) based at the University of Reading. The DTP involves six universities: University of Reading, Cranfield University, University of Surrey, Queen’s University Belfast, Aberystwyth University, and Brunel University London. The DTP will develop the next generation of food scientists utilising techniques within the SCM group and Diamond. In addition, the SCM group was awarded three new doctoral studentships for 2020 that will be shared with the University of Cambridge, Durham University and the University of Manchester. The new cohort of students will join our existing SCM doctoral students associated with the Universities of Pisa (Italy), Surrey and Chalmers, Southampton, College London, Sheffield and Reading. The studentships will support development in infrared nanospectroscopy, SAXS of light activated soft materials and computational methods for modelling 3-dimensional structures of proteins. 2020 will be a transformative year for B22, B23 and I22. B22 will be upgrading its atomic force microscopy (AFM)-IR end station along with a new micro-sample environment for studying catalysis at high temperatures. B23 will be completing its CD-imaging upgrade integrating the new technique fully into the B23 user program. Finally, I22 will complete its BCO project providing world leading capabilities in SAXS based scanning of 2-D and 3-D samples. B21 update B21 studies noncrystalline, randomly oriented particles using high- throughput approaches. SAXS measurements can be made on any type of sample and in any physical state. The life sciences community comprises our largest user group since such measurements provide the opportunity to study biological machines in conditions that are comparable to their liquid, hydrated environment. B21 has been operating with its in-vacuum Eiger 4 M detector for the past year where the entire camera is in a 10 -4 millibar vacuum. The beamline optimised its vacuum configuration improving the instruments’ signal-to- noise whilst allowing sample cell changes to happen within minutes. The new configuration expedites the analysis of non-liquid soft condensed matter samples such as gels and waxes. B21welcomedanewpost-doctoralfellowwhowillbesupportingstructural biologists in lipidic phases while developing automation for the study of semi- solid, gel-like samples. The automation will contribute to a large goal for B21 that will integrate the HPLC and bioSAXS robot fully into the beamline control software enabling full and remote operation of the beamline B22 update TheMultimodeInfraredImagingandMicrospectroscopy(MIRIAM)beamline B22 is used to assess the molecular composition and microscopic spatial distribution of a sample at the highest, optically-achievable resolution in the infrared (IR). B22 operates two end stations for scanning IR spectro-microscopy and IR imaging, with a suite of single and 2-D detectors that seamlessly cover the whole IR range, from near-IR to mid-IR and further into THz. B22 has been used in the analysis of inorganic-organic combinations in biomineralogy or composite materials, chemical degradation in conservation and archaeology, as well as studying live mammalian cells under the IR microprobe for in situ drug response, an important tool in anti-cancer research.This past year, B22 provided insights on a variety of catalytic systems that included enzymes, metal-organic frameworks (MOFs) and zeolite crystals interacting with gas and liquid phase reagents. In 2019, scientists from the University of Oxford (Dr Kylie Vincent) used synchrotron IRmicrospectroscopy to study catalysis of nickel-iron hydrogenases. These are bi-metal enzymes that that have specific CO (carbon-oxygen) and CN (carbon-nitrogen) bonds that can be followed by IR. Dr Vincent’s group invented PFIRE, a method that allowed them to control the enzymes using electrochemistry and follow the catalytic cycle by IR microspectroscopy at B22. Their approach reconciled observations from solid-state approaches, namely X-ray Crystallography (MX), electron paramagnetic resonance and X-ray absorption spectroscopywith solution-state activity studies of enzyme catalysis. ThebeamlinecontinuestoprovidecollaborativecallsforIRnanospectroscopy in photothermal mode (AFM-IR) by synchrotron radiation (SR). This cutting edge method is suitable for molecular analysis of submicron to micron scale organic matter and biomaterials -from mammalian cells to microplastic- with exceptional sub-micron resolution (i.e. up to 100 times below the IRwavelength scale). B22 has approval for a new AFM end station allowing for tapping AFM- IR and scattering-SNOM measurements by SR. The modernisation will improve data acquisition rates and spatial resolution allowing IR nanospectroscopy to be performed at tens of nanometers resolution. This increased sensitivity and spatial resolution will expand B22’s experimental capacity, e.g. surface sciences and the study of thin-films such as organic photovoltaics. B23 update The synchrotron radiation Circular Dichroism (CD) beamline (B23) uses circularly polarised ultraviolet (UV) light to characterise the structure of complex materials in solution and in solid-state films. Many molecular systems have a handedness (chirality) to them akin to our right and left hands and surprisingly, this molecular handedness will differentially absorb light that has been polarised. Specifically to B23, the UV light generated is modulated between right-polarised (spins to the right) and left-polarised (spins to the left). B23 measures precisely the differences in how much a material absorbs the right versus left polarised light through the technique of CD. In thin-films, quantification of CD at 50 micron resolution can inform on how materials prefer to orient themselves and for biological samples, CD spectra can be used to monitor conformational changes, drug binding or instabilities in a protein as a function of temperature, pressure, ionic strength, surfactant, pH, ligand interactions and ageing. B23 is at the forefront of a new CD Imaging (CDi) technology. CDi exploits the highly collimated synchrotron light for scanning thin-films and surfaces of solid materials. Unlike absorption methods, CDi can inform on the chiral supramolecular structure of the material. Last year, B23 had secured funding for a dedicated Mueller-Matrix Polarimeter (MMP) instrument that was delivered and installed in November 2019. The MMP is under commissioning and will see full user schedule later in 2020. CDi measurements require precise knowledge of the sample thickness that often varies throughout the material.To complement the MMP instrument, B23 acquiredtheProFilm3Dprofilometerforprecisesamplethicknessmeasurements. The instrument can provide thickness measurements down to 10 nanometers (1000 times smaller than the thickness of a sheet of paper). Many thin-film materials are made from polymers and these polymers will preferentially form a chiral structure. Currently, the chiral homogeneity throughout the material cannot be interrogated efficiently using non-destructive methods. B23 is the first beamline capable of CDi, the essential tool for the screening of the chiral homogeneity of novel optoelectronic materials for photovoltaic and display systems that are also based on peptides and DNA. Combined with Diamond high-resolution microscopy, B23 is the unique worldwide facility for material science and life sciences. I22 update The Small Angle Scattering and Diffraction beamline (I22) offers combined Small and Wide Angle X-ray Scattering (SAXS and WAXS) studies on a range of low order biological, natural and synthetic samples. I22 excels at providing structural information on partially ordered materials ranging from colloidal nanoparticles and thin-films to large hierarchical structures such as bone. I22 made a major change to its experimental hutch as part of a Beam Conditioning Optics (BCO) upgrade project. The BCO project will significantly improve data quality through a completely embedded microfocus mechanism, providing variable beamsizes, and energy through an evacuated flight tube. In the last phase of the project, the experimental hutch was stripped down to the floor and rebuilt which allowed a significant removal of legacy equipment and cables. A new granite base was installed to provide a solid, temperature- insensitive, anti-vibration platform to host an array of low scatter slits, a laser alignment tool, beam position monitor (QBPM), fast shutter and most importantly, an in-line microscopic viewer of the mounted sample. Samples can now be viewed in real-time with a virtual X-ray beam overlaid on the image. The new optical layout has significantly reduced divergence for microfocus experiments and has provided access to much lower q (scattering vectors) than previously available. The upgrade has been a step-change in mapping experiments particularly examining deformation in bones and eye lenses. Last year, the I22 Principal Beamline Scientist Dr NickTerrill, in collaboration with Professor Michael Rappolt from the School of Food Science and Nutrition at the University of Leeds, was awarded an Engineering and Physical Sciences Research Council (EPSRC) grant to support an offline SAXS facility at Diamond and managed by the SCM Group. The Multi-User Facility for SAXS/WAXS (DL- SAXS) now has an installed Xenocs Xeuss 3.0 instrument operating with an Eiger-2R 1M detector. The facility is under commissioning and will accept a limited number of users in AP28. This instrument will be critical to the SCM Sample Environment Development Laboratory for independent development/ testing of sample environments prior to beamtime. Studying materials under intended use, such as lubricants under frictional strain or simply the stretching of a novel bioengineered material requires bespoke sample environments. Testing these sample environments prior to beamtime drives innovation and optimises the available beamtime.
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